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Short Communication
Bond strength of a dental leucite-based glass ceramicto a resin cement using different silane coupling agents
Tabassom Hooshmanda,n, Jukka P. Matinlinnab, Alireza Keshvadc,Solmaz Eskandariona, Fereshteh Zamania
aDepartment of Dental Biomaterials, School of Dentistry/Research Center for Science and Technology in Medicine, Tehran University of
Medical Sciences, Tehran, IranbDental Materials Science, Faculty of Dentistry, University of Hong Kong, Hong Kong, PR ChinacDepartment of Prosthodontics, School of Clinical Dentistry, Shahed University, Tehran, Iran
a r t i c l e i n f o
Article history:
Received 30 May 2012
Received in revised form
24 August 2012
Accepted 27 August 2012
Available online 1 September 2012
Keywords:
Bond strength
Leucite-based dental ceramic
Resin cement
Silane coupling agent
nt matter & 2012 Elsevie.1016/j.jmbbm.2012.08.02
hor. Tel.: þ98 21 [email protected]
a b s t r a c t
Aim: To evaluate the effect of different types of novel silane coupling agents with two
concentrations on the micro-tensile bond strength of a dental glass ceramic with leucite
crystals to a dual-cured resin cement using an optimized method of silane application.
Methods: Leucite-reinforced feldspathic ceramic blocks were fabricated, wet ground and
cleansed. The bonding ceramic surfaces were treated with different organosilane solutions
as follows: Control silane: Monobond S; methacryloxypropyltrimethoxy silane and experi-
mental silanes with two concentrations (1.0 and 2.5 vol%): amino, isocyanate, styryl, and
acrylate silanes. The silane application method consisted of brush application, hot air
drying followed by rinsing with hot water and drying. Then a thin layer of an unfilled resin
and a dual-cured resin cement was light-cured on the ceramic surfaces. The resin–ceramic
blocks were stored in distilled water at 37 1C for 24 h and sectioned to produce beam
specimens (n¼17) with a 1.0 mm2 cross-sectional area. Specimens were then subjected to
thermocycling and tested in a micro-tensile tester device. Data were analyzed using
analysis of variance and Tamhane post-hoc test.
Results: The mean micro-tensile bond strength value for the styryl silane was significantly
higher (Po0.05) than the other types of silanes except for the Monobond S. The mean bond
strength values for isocyanate silanes were significantly lower than the other silanes tested
(Po0.05). No statistically significant difference in the bond strength between the 1.0 and
2.5 vol% of experimental silanes was observed (P40.05).
Conclusions: The micro-tensile bond strength of the leucite-based dental glass ceramic to a
resin cement was affected by the type of silane coupling agent and not by the concentra-
tion of silane solutions. The best bond strength overall was achieved by methacrylox-
ypropyltrimethoxysilane and experimental styryl silane solutions.
& 2012 Elsevier Ltd. All rights reserved.
r Ltd. All rights reserved.0
; fax: þ98 21 88081699.c.ir (T. Hooshmand).
j o u r n a l o f t h e m e c h a n i c a l b e h a v i o r o f b i o m e d i c a l m a t e r i a l s 1 7 ( 2 0 1 3 ) 3 2 7 – 3 3 2328
1. Introduction
Clinical performance of metal-free fixed-partial-dentures
(FPD) made of silica-based ceramics, either in the forms of
inlays, onlays or laminate veneers, substantially relies on the
adhesion of the resin cements to ceramic restorations and
tooth tissues. For the adhesive cementation procedures, the
silica-based ceramic surfaces are usually etched by hydro-
fluoric acid (HF) with or without gritblasting for mechanical
interlocking, and then silanated for chemical bonding. How-
ever, a major concern exists about the use of HF acid etching
due to its hazardous effects on health (Meldrum, 1999) and
possible deleterious effects on ceramic strength (Hussain
et al., 1979; Hooshmand et al., 2002). Still research continues
in introducing effective silane solutions to optimize the
chemical bond provided by silanes such that there would be
no need for the HF acid etching of the ceramic surfaces.
Silane coupling agents with the general formula R–Si–(OR0)3are capable of forming bonds with both inorganic and organic
surfaces. The organo-functional group (R) is chosen for
reactivity with the organic matrix and R is most frequently
a vinylic group,, while the hydrolyzable groups (R0) are
intermediates in the formation of silanol groups (Si–OH) for
bonding to mineral (e.g., ceramic) surfaces. They are usually
methoxy groups because they are kinetically favourbale for a
rapid hydrolysis during activation of the silane coupling
agent. The most commonly used silane in dental applications
is g-methacryloxypropyltrimethoxysilane (g-MPTS) which
can then be polymerized with the monomers of a resin
composite system.
Recent studies have shown that experimental silane mono-
mer primers can significantly increase the bond strengths
between resins and zirconia ceramic (Aboushelib et al., 2008,
2009; Matinlinna and Lassila, 2011). The rationale behind
applying experimental silane primers is that the presence
of specific organofunctional groups, such as an aromatic
reactive styryl, isocyanato (with the –N¼C¼O functionality),
glycidoxy (with epoxy ring), or acrylate, may improve the
spatial compatibility of the silane molecule (Matinlinna et al.,
2005a; Matinlinna et al., 2007; Heikkinen et al., 2009). This
steric improvement may also increase the reactivity of silane
monomers by enabling polymerization reactions between
methacrylate, acrylate and styryl groups and, on the other
hand, with methacrylate and phosphate ester groups in
resin-composite.
In our previous studies, the macro-tensile bond strength
and interfacial fracture toughness of smooth and roughened
leucite-based ceramic surfaces bonded to a luting resin using
an optimized silane treatment method was investigated
(Hooshmand et al., 2002; Moharamzadeh et al., 2008). It was
concluded that mechanical interlocking by gritblasting the
leucite ceramic surfaces could be sufficient with no need for
HF acid etching the ceramic surfaces when an appropriate
silane application procedure was used. A possible explana-
tion for these observations was that the silane application
procedure used resulted in the formation of a monolayer of
the silane coupling agent by washing away any unreacted
silane primer components, rather than the formation of
interphase layer as described by Ishida and Koenig (1980).
In addition, it has been found that the interfacial fracture
toughness for a lithium disilicate glass ceramic system was
affected by the surface treatment and type of luting agent
(Hooshmand et al., 2012). The optimized silane treatment
method was only capable of eliminating the need for HF acid
etching of ceramic surfaces bonded to one type of dual-cured
resin cements.
The purpose of this study was to evaluate the effect of
different types of novel silane coupling agents with two
concentrations on the micro-tensile bond strength of a dental
glass ceramic with leucite crystals to a dual-cured resin
cement using an optimized method of silane application.
2. Materials and methods
Eighteen leucite-reinforced feldspathic ceramic blocks
(Ceramco II, Dentsply) in dimensional of 6�6�6 mm3 were
fabricated according to the manufacturer’s instructions. The
ceramic blocks were ground on wet 400–800 grit SiC papers
and then cleansed in distilled water in an ultrasonic device
for 15 min. The experimental silane primers were used at
1.0% and 2.5% (v/v) in a standard solution of 95.0% (v/v)
ethanol and deionized water (Milli-Q purification system,
Millipore) that had been adjusted to pH 4.5 with 1 M acetic
acid. The solution was first allowed to stabilize for 24 h and
then silane monomer was added and allowed to activate for
1 h at room temperature. The chemical compositions of
silane coupling agents are shown in Fig. 1. The bonding
ceramic block surfaces were then treated with different
silane solutions (n¼2) as follows:
Group 1: (commercial as control): Monobond S; (Lot No.,
M01959; Ivoclar-Vivadent, Liechtenstein), 3-methacryloxy-
propyltrimethoxysilane (MPTS silane).
Group 2: Experimental 3-Acryloyloxypropyltrimethoxy-
silane (ACPS).
Group 3: Experimental 3-Isocyanatopropyltriethoxysilane
(ICS).
Group 4: Experimental Styrylethyltrimethoxysilane (STYRX).
Group 5: Experimental 3-(N-allylamino)propyltrimethoxy-
silane (ALAP).
Each experimental silane group was applied in two differ-
ent concentration of 1.0 and 2.5 percent by volume. The
silane application method consisted of brush application for
60 s, hot air drying at 5075 1C with a hair drier for 15 s
followed by rinsing with hot water for 15 s and drying again
with hot air for 30 s. Then a thin layer of an unfilled resin
(HelioBond, Lot No., J14889; Ivoclar-Vivadent, Liechtenstein)
was applied on the silane-treated ceramic surfaces and light-
cured for 20 s.
The ceramic blocks were then transferred to a custom-
made teflon mold in size of 6�6�12 mm3 and a dual-cured
resin cement (Variolink II, Lot No., K37003; Ivoclar-Vivadent)
was added and light-cured incrementally on the ceramic
surfaces using a halogen curing light at a light intensity of
800 mW/cm2 for 40 s. The specimens were also post-cured for
an additional of 40 s in different directions.
ResinCeramic
Fig. 2 – (a) Micro-tensile bond strength tester and (b)
schematic picture of microbar specimen fixation.
CH3
CH2=C-C-O-CH2CH2CH2-Si-OCH3
OCH3
OCH3
H2CO Si
OCH3
O
O
CH3
CH3O
OC2H5
OC2H5C2H5O
SiN
C
O
H2C Si
O
OO
CH3
CH3
CH3
H2C
N
Si
O
O
OCH3
CH3H3C
H
Fig. 1 – (a) methacryloxypropyltrimethoxysilane (MPTS); (b) 3-acryloyloxypropyltrimethoxysilane (ACPS);
(c) 3-isocyanatopropyltriethoxysilane (ICS); (d) styrylethyltrimethoxysilane (STYRX) and (e) 3-(N allylamino)
propyltrimethoxysilane (ALAP).
j o u r n a l o f t h e m e c h a n i c a l b e h a v i o r o f b i o m e d i c a l m a t e r i a l s 1 7 ( 2 0 1 3 ) 3 2 7 – 3 3 2 329
The ceramic–resin cement blocks were kept in distilled water
at 37 1C for 24 h and then were cut using a slow speed diamond
saw (Isomet, Buehler, Lake Bluff, IL, USA) under water cooling.
The sectioning continued until 1 mm remained to keep the
specimen in a fixed position. The ceramic–resin cement block
was then rotated 901 and the procedure repeated. The peripheral
slices were disregarded in case the results could be influenced by
either excess or insufficient amount of resin cement at the
interface. A total of 17 bar specimens per group approximately
1 mm2 in cross section with bonded ceramic to resin cement
(6 mm in height each) were obtained.
The spemines were then subjected to thermocycling for 5000
cycles between 5 and 55 1C water baths (immersion time 20 s;
transfer time 20 s). Each microbar was glued with cyanoacrylate
and fixed in a micro-tensile tester device (Bisco micro-tensile
tester, USA) as shown in Fig. 2. The tensile load was applied at a
cross-head speed of 0.5 mm/min until fracture. The load at
failure in Newtons was recorded, and the fragments of the
specimen were carefully removed from the fixture with a scalpel
blade. The cross-sectional area at the site of fracture was
measured to calculate the bond strength at failure in MPa. The
debonded bar specimens were analyzed for mode of failures
with a stereomicroscope (Olympus, SZX 12, Tokyo, Japan).
Data were analyzed using two-way ANOVA to assess
possible differences and interaction between between type
of silane and silane concentration. One-way analysis of
variance and Tamhane test were used for post-hoc compar-
isons between experimental groups. The level of significance
was set at Po0.05 using statistical software (SPSS 11 for
Windows; SPSS Inc., Chicago, IL, USA).
3. Results
The description of micro-tensile bond strength data are
presented numerically in Table 1 and graphically in Fig. 3.
The interaction between silanes and silane concentration
was significant (Po0.0001), thus, one-way analysis of variance
and Tamhane test due to the non-homogeneity of variances
were used for post-hoc comparisons between experimental
groups.
The results showed that the highest mean micro-tensile
bond strength value was obtained for the 2.5% styryl silane
(STYRX) followed by Monobond S (MPTS silane). In addition,
Table 1 – Statistical description of micro-tensile bond strength data for different groups.
Mean (MPa) SDa SEb Statistical differencen
Monobond-S 26.56 2.88 0.69 a
1.0% ACPS 16.13 2.84 0.68 b
2.5% ACPS 15.90 3.05 0.74 b
1.0% ICS 11.14 3.02 0.73 c
2.5% ICS 12.54 2.32 0.56 c
1.0% STYRX 22.54 9.11 2.20 a, b and d
2.5% STYRX 31.80 9.30 2.25 a
1.0% ALAP 21.95 3.13 0.76 d
2.5% ALAP 21.91 3.07 0.74 d
a Standard deviation.b Standard error.n Identical letters indicate statistically no significant difference between groups (Po0.05).
Fig. 3 – Micro-tensile bond strengths data for different silane
solutions.
j o u r n a l o f t h e m e c h a n i c a l b e h a v i o r o f b i o m e d i c a l m a t e r i a l s 1 7 ( 2 0 1 3 ) 3 2 7 – 3 3 2330
the mean micro-tensile bond strength value for the 2.5%
styryl silane (STYRX) was significantly higher (Po0.05) than
the other types of silanes, except for the Monobond S and
1.0% styryl silanes (P40.05). The mean micro-tensile bond
strength value for the Monobond S (control) was significantly
higher (Po0.05) than the other types of silanes, except for the
styryl silanes (1.0% and 2.5% STYRX).
The lowest mean micro-tensile bond strength values were
obtained for the isocyanate silanes (1.0% and 2.5% ICS) which
were significantly lower than the other silanes tested
(Po0.05).
No statistically significant difference in the mean micro-
tensile bond strength between the 1.0 and 2.5 vol% of experi-
mental silanes was observed (P40.05).
The predominant mode of failure for all the groups tested
was interfacial adhesive fracture (410 out of 17 specimens).
The remaining failures were mixed ceramic–resin fracture.
4. Discussion
The degree of bond strength enhancement of resin to dental
ceramic mainly depends on the bond of silane to the ceramic
surface. In the present study, the bonding effectiveness of a
leucite-reinforced glass ceramic to a dual-cured resin cement
using different types of experimental silane solutions with
two concentrations were compared with that of a commercial
methacryloxypropyltrimethoxysilane. We performed the
micro-tensile bond strength test with small specimen size
of 1 mm2 because the validity of expressing bond strength in
terms of nominal (i.e., average) stress in macro-bond strength
tests has been questioned due to the heterogeneity of the
stress distribution at the bonded interface (Van Noort et al.,
1989, 1991). The need for new test methods to overcome
these limitations has led to the use of specimens with small
bonding areas (i.e., below 2 mm2), in the so-called micro-
tensile and micro-shear bond strength tests (Sano et al.,
1994). Smaller test specimens are ‘stronger’ than larger ones
due to the lower probability of having a critical sized defect
present and aligned in a crack opening orientation relative to
the applied load (Armstrong et al., 2010).
The silane treatment procedure used in the present study
was introduced previously (Hooshmand et al., 2002;
Moharamzadeh et al., 2008) using an optimized method for
ceramic–resin bonding such that a chemisorbed monolayer of
the silane coupling agent can be created with no need for HF
acid etching. We did not make any additional mechanical
interlocking by gritblasting or HF acid etching in order to
assess the unique impact of chemical adhesion by silane
coupling agents.
We may say that from this in vitro study it is quite clear
that different functional silanes have a significant impact on
the bond strength between resin composite and leucite-
reinforced dental ceramics. In our study, we used thermo-
cycling for artificial aging which is widely used as an accepted
laboratory method. We did not measure the initial bond
strength in this study because we aimed showing differences
in the micro-tensile bond strengths after thermocycling.
The literature demonstrate that different results in promoting
adhesion are obtained according to the type of silane used
(Hooshmand et al., 2004; Anagnostopoulos et al., 1993; Pratt
et al., 1989). Several silane coupling agent systems are available
and they are categorized into pre-hydrolyzed single liquid silane
primer and 2- or 3- liquid silane primers. Those supplied as a
single component system are previously hydrolyzed and the
silane content is usually about 1–5 vol%. For those supplied as 2
separate components, the hydrolysis occurs moments before
application and after mixing the two components.
j o u r n a l o f t h e m e c h a n i c a l b e h a v i o r o f b i o m e d i c a l m a t e r i a l s 1 7 ( 2 0 1 3 ) 3 2 7 – 3 3 2 331
Based on the statistical analysis, except for one experi-
mental 2.5 vol% styrylethyltrimethoxysilane (STYRX), other
silane primers resulted in lower micro-tensile bond strengths
than that of the control MPTS silane. It has been reported that
the use of styryl silane (STYRX) in experimental dimethacry-
late thermoset composites has produced the highest moduli
(Wilson and Antonucci, 2006). This was explained by the high
reactivity of STYRX. In the current study, a 2.5% conentration
of styryl silane produced 19.7% higher bond strengths, where
as the dilute 1.0% styryl-based primer produced 15% lower
bond strength than that of the control silane, although not
statistically different.
It has been reported that pre-acitivated dental silanes may
produce differences in adhesion promotion (Matinlinna et al.,
2006b). Monobond S is a single-phase and pre-activated silane
solution based on the 3-methacryloxyprophyltrimethoxy silane
molecules. It was selected as the control silane because it is
ready for immediate use as supplied by the manufacture. In
addition, Monobond S produced significantly higher bonding
than another dental silane product after artificial aging of the
resin bonded Ti specimens (Matinlinna et al., 2005b). The high
bonding efficacy observed for the Monobond S in this study is in
agreement with the results of our previous study (Hooshmand
et al., 2004) in which a pre-activated silane solution based on
g-MPTS did not deteriorate when stored up to one year.
The experimental 1.0 or 2.5 vol% 3-Isocyanatopropyltriethoxy-
silane (ICS) silane solutions did not improve adhesion between
the ceramic and resin cement in the present study. The lowest
micro-tensile bond strengths were obtained by ICS silanization
in both concentrations. This has been also confirmed by a
previous study (Matinlinna et al., 2004b). The effect of silane
concentration on the titanium surface treatment was investi-
gated in a study done by Matinlinna et al. (2008). They found that
a novel silane system with an optimal concentration of the
cross-linking silane of 1.0% as opposed to the 0.1%, 0.2%, 0.3%,
and 0.5% could produce significantly higher shear bond strength
between silica-coated titanium and a resin cement when com-
pared to a pre-activated silane product. On the contrary, it was
reported that 0.1 vol% experimental ICS silane primer enhanced
the resin to titanium bond strength significantly higher than that
of a 1.0 vol% ICS primer, a finding that supports the use of
relatively dilute primers (Matinlinna et al., 2005a). However,
silane solutions with greater concentrations in the present study
demonstrated comparable micro-tensile bond strength values
between the leucite-reinforced feldspathic ceramic and resin
cement with that of lower concentrations.
Surprisingly, both ALAP and ACPS silane primers exhibited
almost no significant improvement in the bond strength
regardless of the silane concentration. According to the
results obtained by another study (Matinlinna and Lassila,
2011), ACPS has produced significantly higher bond strengths
than experimental MPTS silane primer. On the other hand,
one study using 2.0 vol% experimental silanes on silica-
coated Ti substrate found that MPTS and ACPS did not differ
statistically from each other for their adhesion promotion
ability (Matinlinna et al., 2007). On the resin–zirconia bonding,
an in vitro study suggested that ACPS and MPTS perfomed
equally well in adhesion promotion (Matinlinna et al., 2006a).
It should be noted that results from these studies have been
obtained on different types of substrates, resin cements, and
test parameters than that of used in the present study. Thus,
comparison and interpretation of results are difficult.
It is also essential to note that ceramic surfaces and silica-
coated metal surfaces exhibit chemically and topologically
different surfaces, and are definitely not equivalent or com-
parable. It has been suggested that the surface nature of the
inorganic substrate or filler must be considered in the selec-
tion of a silane coupling agent (Matinlinna et al., 2004a; Shen
et al., 2004). Other factors to be considered include the type
and availability of surface hydroxyl groups (silanol vs
adsorbed water, hydrated ions, etc.), hydrolytic stability of
the oxane bond that forms, number of active hydroxyl groups
per unit area of substrate, surface reactivity and chemical/
physical properties of the silane and silanization conditions
(silane concentration, pH, temperature, type of catalysis,
method of silane application, etc.).
To our knowledge, there is no other experiment that has
evaluated the resin to leucite-reinforced glass ceramic bond
strength using the novel experimental silane primers in this
study, without HF acid pretratment. Finally, it should be noted
that there are some limitations to this study. The microbar
specimens were cut from very limited number of bonded
ceramic–resin blocks, it is possible that different results could
be obtained if the sample size was increased. These should be
considered when the data are compared because ceramic
testing is statistical in nature. Besides, the results obtained
from this in vitro study cannot necessarily be extrapolated to
the clinical situation because of the complex oral environ-
ment and further long-term storage time or clinical studies
on the bonding efficacy of these organosilanes are required.
5. Conclusions
The findings in this in vitro study may indicate that the
micro-tensile bond strength of a dental leucite-based glass
ceramic to a dual-cured resin cement is affected by the type
of silane coupling agent and not by the concentration (1 or
2.5 vol%) of silane solutions. The freshly made styryl silane
may be as effective as pre-activated methacryloxypropyltri-
methoxysilane in promoting bond strength.
Acknowledgments
This study was supported by Research Center for Science and
Technology in Medicine (Tehran University of Medical
Sciences). We thank Dr. M.J. Kharazifard for his invaluable
assistance in the statistical analysis.
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